Buchi KjelMaster K-375 User manual

Type
User manual
KjelMaster K-375 with KjelSampler K-376 / K-377
Operation Manual
11593514Fen
Imprint
Product Identification:
Operation Manual (Original), KjelMaster K-375 with KjelSampler K-376 / K-377
11593514F en
Publication date: 04.2023
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH-9230 Flawil 1
E-Mail: quality@buchi.com
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experience; espe-
cially in respect to structure, illustrations and technical detail.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purpos-
es, nor made available to third parties. The manufacture of any component with the aid of this manual without
prior written agreement is also prohibited.
Document History
Index Date Author Changes
A 25/MAY/2012 NAGG Initial version
B 16/JUL/2013 NAGG First revised version
C 17/NOV/2014 HILS/BRUS Second revised version
(update colorimetric titration)
D 28/APR/2016 HILS Removal of Declaration of Conformity
E 12/DEC/2018 HOES Third revised version
(update colorimetric titration)
F 25/APR/2023 SALN Update technical tata
Read this manual carefully before installing and running your system and note the safety precautions in chapter 2 in
particular. Store the manual in the immediate vicinity of the instrument, so that it can be consulted at any time.
No technical modifications may be made to the device without the prior written agreement of BUCHI. Unauthorized
modifications may affect the system safety or result in accidents.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes,
nor made available to third parties. The manufacture of any component with the aid of this manual without prior
written agreement is also prohibited.
If you need another language version of this manual, you can download it at
www.buchi.com.
Table of contents
5K-375 / K-376 / K-377 Operation Manual, Version F
Table of contents
1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
1.1 Trademarks 9
1.2 Abbreviations 9
2 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
2.1 User qualification 10
2.2 Proper use 10
2.3 Improper use 10
2.4 Safety warnings and safety signs used in this manual 11
2.5 Product safety 12
2.5.1 General hazards 12
2.5.2 Instrument-related hazards 13
2.5.3 Other hazards 14
2.5.4 Personal protective equipment 14
2.5.5 Built-in safety elements and measures 15
2.6 General safety rules 16
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3.1 Scope of delivery 17
3.1.1 Basic devices 17
3.1.2 Standard accessories for K-375 19
3.1.3 Standard accessories for K-376 / K-377 21
3.1.4 Operation Manuals for K-375 22
3.1.5 Optional accessories K-375 23
3.1.6 Optional accessories K-376 / K-377 25
3.2 Technical data overview 26
3.2.1 Technical data KjelMaster K-375 and KjelSampler K-376 / K-377 26
3.2.2 Technical data titrator 27
3.3 Determination parameters 28
3.4 Information on type plate 29
3.4.1 Titrator module and dosing unit 29
3.4.2 Material on the K-375 29
3.4.3 Material on the K-376 / K-377 30
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
4.1 Device overview 31
4.1.1 Opening the service door 32
4.2 Functional principle of KjelMaster System K-375 / K-376 / K-377 33
4.3 Standby function 35
4.4 System preparation 35
4.4.1 Preheating 35
4.4.2 Priming 35
4.4.3 Cleaning 35
4.4.4 Aspiration 35
4.5 Distillation and titration 36
4.5.1 Distillation and Titration Options 36
4.5.2 Distillation Mode 36
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6K-375 / K-376 / K-377 Operation Manual, Version F
4.5.3 Titration Type 36
4.5.4 Sensor Type 36
4.5.5 Titration Mode 37
4.5.6 Measuring Mode 37
4.5.7 Titration Algorithm 37
4.5.8 Determination Mode 37
4.6 Different methods 38
4.7 Blank values 38
4.7.1 Blanks 38
4.7.2 Control blanks 39
4.8 Reference substances 39
4.9 Indicator for colorimetric titration 40
4.10 Result Groups 40
4.11 Explanation of alkaline direct distillation 41
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
5.1 Installation site 43
5.2 Electrical connections 44
5.2.1 Connections of the KjelMaster K-375 44
5.2.2 Connections of the K-376 / K-377 45
5.3 Transfer connection K-376 / K-377 to K-375 46
5.3.1 Connecting the K-376 to the K-375 46
5.3.2 Connecting the transfer hoses of the K-377 48
5.4 Reagent/water and waste connections 49
5.5 Buret unit for titrant 51
5.6 Positioning of the dosing tip 53
5.7 Storage tank connection 53
5.8 Level sensors 54
5.9 Installation of the titration sensor 56
5.9.1 Potentiometric sensor 56
5.9.2 Colorimetric sensor 56
5.10 Connections to peripheral devices 57
5.10.1 Connecting a printer 57
5.10.2 Connecting a network cable 57
5.10.3 Connecting a KjelSampler K-376 or K-377 57
5.10.4 Connecting a balance 57
5.10.5 Connecting a bar code reader 58
5.10.6 External dosing unit for back titration 58
5.11 Preparing the system 58
5.11.1 Preparing the software 58
5.11.2 Preparing the hardware 59
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .60
6.1 The operating principle 60
6.2 The home screen 60
6.2.1 The title bar 62
6.2.2 The bottom bar 62
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7K-375 / K-376 / K-377 Operation Manual, Version F
6.2.3 System status icons 63
6.3 User concept 63
6.4 Editable and non-editable menu items 63
6.5 The status view 65
6.5.1 RESULT display 66
6.5.2 CHART display 67
6.6 Determination 67
6.6.1 System Preparation 69
Single Sample 77
6.6.3 Sample Lists 79
6.6.4 Sequences 84
6.7 Results 92
6.7.1 Result groups 92
6.7.2 Last Results 94
6.7.3 Blank Correction 95
6.8 Determination Parameters 99
6.8.1 Methods 99
6.8.2 Volumetric Solutions 108
6.8.3 Reference Substances 109
6.9 Device 110
6.9.1 Settings 110
6.9.2 Utilities 117
6.9.3 Diagnostics 118
6.9.4 Logout 119
7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 119
7.1 Daily maintenance 120
7.1.1 Before sample determination (potentiometry) 120
7.1.2 Before sample determination (colorimetry) 121
7.1.3 After sample determination 122
7.1.4 pH electrode 122
7.1.5 Filling boric acid into receiving vessel after last sample of rack was determined
(potentiometry only) 123
7.1.6 Sample tube cleaning 124
7.2 Weekly maintenance 125
7.2.1 Cleaning the housing 125
7.2.2 Cleaning the titrator 125
7.2.3 Cleaning the glass parts of the dosing unit 125
7.2.4 Cleaning the dip tube of the KjelSampler 125
7.2.5 Device monitoring 126
7.2.6 Cleaning colorimetric sensor and mesh 127
7.3 Monthly maintenance 127
7.3.1 Calibrating the pump 127
7.3.2 Checking the distillate amount 129
7.3.3 Inspecting the buret 130
7.3.4 Inspecting the titrator 130
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8K-375 / K-376 / K-377 Operation Manual, Version F
7.3.5 Inspecting the sample tubes 130
7.4 Half-yearly maintenance 132
7.4.1 K-375 Sealing between sample tube and splash protector 132
7.4.2 K-376 / K-377 dip tube and sealing cap 133
7.4.3 Replacing the splash protector 134
7.5 Yearly maintenance 136
7.5.1 Replacement of wear parts 136
7.5.2 Decalcification of the steam generator 137
7.5.3 Replacement of the sodium hydroxide pump 137
7.5.3 Replacement of the wave spring 138
7.6 Replace every two years 139
7.6.1 Replacement of the transfer connection 139
7.7 Maintenance work if required 141
7.7.1 Changing the buret tip 141
7.7.2 Cleaning the pH electrode 141
7.7.3 Replacing the buret 142
7.7.4 Cleaning the splash protector and the rubber seal 142
7.7.5 Glass parts 142
7.7.6 Troubleshooting the dosing unit 143
7.7.7 Adjusting the sample tube holder 143
7.8 Customer service 144
8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 145
8.1 Problems that may occur 145
8.2 Error messages on the display of the K-375 149
8.3 Eliminating errors of the KjelSampler K-376 / K-377 153
8.4 Eliminating errors of the titrator 154
9 Taking out of operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 155
9.1 Emptying the steam generator 155
9.2 Emptying the buret of the titrator 156
9.3 Storage/shipping 156
9.4 Disposal 156
10 Spare parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 157
10.1 Spare parts K-375 157
10.2 Spare parts K-376 / K-377 160
10.3 Hosing connection scheme Kjeldahl Sampler System K-375 / K-376 160
11 Declarations and requirements 161
11.1 FCC requirements (for USA and Canada) 161
1 About this manual
9K-375 / K-376 / K-377 Operation Manual, Version F
1 About this manual
This manual describes the KjelMaster System K-375 / K-376 / K-377 and provides all information
required for its safe operation and to maintain it in good working order.
It is addressed to laboratory personnel in particular.
NOTE
The symbols pertaining to safety (DANGER, CAUTION and WARNING) are explained in chapter 2.
1.1 Trademarks
DURAN® is a registered trademark of the SCHOTT AG.
Nylflex® is a registered trademark of the Pedex & Co. GmbH.
1.2 Abbreviations
CSM: Chopped Strand Mat
ETFE: Polytetrafluorethylene
FEP: Fluorinated Ethylene Propylene
KCI: Potassium chloride
PCTFE: Polychlorotrifluoroethylene
PMMA: Polymethyl methacrylate
POM: Polyoxymethylene
PP: Polypropylene
PTFE: Ethylenetetrafluoroethylene
PUR: Polyurethane
UV: Ultraviolet
EPDM: Ethylene propylene diene monomer
PVDF: polyvinylidene difluoride
PA: Polyamides
2 Safety
K-375 / K-376 / K-377 Operation Manual, Version F
10
2 Safety
This chapter points out the safety concept of the device and contains general rules of behavior and
warnings from hazards concerning the use of the product.
The safety of users and personnel can only be ensured if these safety instructions and the safety
related warnings in the individual chapters are strictly observed and followed. Therefore, the manual
must always be available to all persons performing the tasks described herein.
2.1 User qualification
The device may only be used by laboratory personnel and other persons who on account of training
or professional experience have an overview of the dangers which can develop when
operating the instrument.
Personnel without this training or persons who are currently being trained require careful instruction.
The present Operation Manual serves as the basis for this.
2.2 Proper use
The device has been designed and built for laboratories. It serves for nitrogen determination
according to Kjeldahl. The KjelMaster K-375 as stand-alone device may also be used for distillations
of steam-volatile substances.
2.3 Improper use
Applications not mentioned above are improper. Also applications which do not comply with the tech-
nical data are considered improper.
! Danger
During any improper use, the effectiveness of the protection systems of the devices
can be affected.
Avoid any improper use of the devices!
The operator bears the sole risk for any damages caused by such improper use.
The following uses are expressly forbidden:
Use of the device in rooms which require ex-protected devices.
Use on samples which can explode or inflame (e.g.: explosives, etc.) due to shock, friction, heat
or spark formation.
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2.4 Safety warnings and safety signs used in this manual
DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of
hazard seriousness of risks related to personal injury and property damage. All signal words, which
are related to personal injury are accompanied by the general safety sign.
For your safety it is important to read and fully understand the table below with the different signal
words and their definitions!
Sign Signal word Definition Risk level
DANGER Indicates a hazardous situation which, if not
avoided, will result in death or serious injury. ★★★★
WARNING Indicates a hazardous situation which, if not
avoided, may result in serious injury or death. ★★★☆
CAUTION Indicates a hazardous situation which, if not
avoided, may result in minor or moderate injury. ★★☆☆
NOTICE Indicates possible material damage, but no prac-
tices related to personal injury. ☆☆☆☆
Supplementary safety information symbols may be placed in a rectangular panel on the left to the
signal word and the supplementary text (see example below).
Space for
supplemen-
tary safety
information
symbols.
SIGNAL WORD
Supplementary text, describing the kind and level of hazard / risk seriousness.
List of measures to avoid the herein described, hazard or hazardous situation.
...
...
Table of supplementary safety information symbols
The reference list below incorporates all safety information symbols used in this manual and their
meaning.
Warning safety symbols
Symbol Meaning Symbol Meaning
General warning Corrosive hazard
Electrical hazard Flammable
Biohazard Explosive environment
Broken glass Inhalation harmful
2 Safety
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Symbol Meaning Symbol Meaning
Device damage Hot surface
Hand bruising Magnet
Mandatory safety symbols
Symbol Meaning Symbol Meaning
Wear protective goggles Wear protective clothes
Wear protective gloves Heavy load, lift with assistance
Additional user information
Paragraphs starting with NOTE transport helpful information for working with the device / software or
its supplementaries. NOTEs are not related to any kind of hazard or damage (see following example).
NOTE
Useful tips for the easy operation of the instrument / software.
2.5 Product safety
The device is designed and built in accordance with current state-of-the-art technology. Neverthe-
less, risks to users, property, and the environment can arise when the device is used carelessly or
improperly.
The manufacturer has determined residual dangers emanating from the instrument
if the device is operated by insufficiently trained personnel.
if the device is not operated according to its proper use.
Appropriate warnings in this manual serve to make the user alert to these residual dangers.
2.5.1 General hazards
The following safety messages show hazards of general kind which may occur when handling the
instrument. The user shall observe all listed counter measures in order to achieve and maintain the
lowest possible level of hazard.
Additional warning messages can be found whenever actions and situations described in this manual
are related to situational hazards.
2 Safety
K-375 / K-376 / K-377 Operation Manual, Version F
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Danger
Death or serious injuries by use in explosive environments.
Do not store or operate the device in explosive environments.
Remove all sources of flammable vapors.
Do not store chemicals in the vicinity of the device.
Caution
Risk of minor or moderate cuts by sharp edges.
Do not touch defective or broken glassware with bare hands.
Do not touch thin metal edges.
Notice
Risk of device damage by liquids or mechanical shocks.
Do not spill liquids over the device or its components.
Do not drop the device or its components.
Keep external vibrations away from the instrument.
2.5.2 Instrument-related hazards
! CAUTION
Risk of injury.
Never touch the surface of the touch screen with pointed or sharp objects!
Otherwise the screen might get damaged and splinter.
! CAUTION
Risk of burns by hot surface. Surface temperature exceeds 60 °C.
Do not touch hot surfaces of the instrument.
! CAUTION
Risk of pinch point injuries.
In order to avoid injuries to the hands and fingers the K-376 and K-377 Kjel-
Samplers may not be manipulated during the moving action of the sampler
arm.
! CAUTION
Risk of burns by hot steam.
The system works with hot steam. Avoid any contact with hot steam.
2 Safety
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! DANGER
Risk of chemical burns by corrosives.
Wear laboratory coat, protective gloves and protective goggles at all times.
! DANGER
Risk of chemical burns by corrosives.
During operation the sample tube contains either strong acid or strong base. In
case the sample tube brakes, the content of the sample tube is collected in the
drip tray on the bottom of the housing. Wear laboratory coat protective gloves
and protective goggles when emptying the drip tray.
2.5.3 Other hazards
Fundamental dangers arise from.
acids and lye
flammable gases or solvent fumes in the direct vicinity of the instrument
damaged glass parts
insufficient distance between the device and the wall (see chapter 5.1, Installation site)
burns caused by contact with hot glass parts
burns caused by contact with steam at the waste-outlet
defective transfer tube: escape of steam and/or sulfuric acid
2.5.4 Personal protective equipment
Always wear personal protective equipment such as protective eye goggles, protective clothing and
gloves. The personal protective equipment must meet all requirements of all data sheets for the
chemicals used. These instructions are an important part of the K-375, K-376 and K-377 and must be
made available at all times to the operating personnel at the place where the equipment is deployed.
This also applies to additional language versions of these instructions, which can be reordered sepa-
rately.
2 Safety
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! WARNING
Serious chemical burns by corrosives.
Observe all data sheets of the used chemicals.
Handle corrosives in well ventilated environments only.
Always wear protective goggles.
Always wear protective gloves.
Always wear protective clothes.
Do not use damaged glassware.
2.5.5 Built-in safety elements and measures
The KjelMaster K-375 has monitored protective doors which prevent a distillation to start while a door is
open. A running distillation is immediately interrupted when a door is opened. The dosing of reagents is
also immediately stopped.
The sample changers K-376 / K-377 have monitored protective shields. Running a sample changer with
opened shield is impossible. For the K-377 only the shield of the tray, that is currently not in use can be
opened.
K-375:
Protective door: Safety appliance to protect users from burns at the splash protector (distillation
area) which is hot during distillation.
Protective door sensors: Prevents to start a distillation with the protective doors open and stops the
distillation as soon as a protective door is opened during the process.
Sample tube sensor: Prevents to start a distillation without a sample tube inserted.
Service door sensor/switch: Electrical power is disconnected immediately when the service door is
opened, thus preventing electrical shock during maintenance.
K-376:
Protective shield with sensor/switch: As soon as the shield is opened an alarm sound is triggered
and any movement of the arm is stopped.
K-377:
Protective shield with sensor/switch: As soon as the shield of the tray in use is opened an alarms
sound is triggered and any movement of the arm is stopped. (The shield of the respective tray that
is not operated can still be opened without any restrictions.)
2 Safety
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2.6 General safety rules
Responsibility of the operator
The head of the laboratory is responsible for training his/her personnel.
The operator shall inform the manufacturer without delay of any safety-related incidents which might
occur during operation of the device or its accessories. Legal regulations, such as local, state and
federal laws applying to the device or its accessories must be strictly followed.
Duty of maintenance and care
The operator is responsible for the proper condition of instrument. This includes maintenance, service
and repair jobs that are performed on schedule by authorized personnel only.
Spare parts to be used
Use only genuine consumables and spare parts for maintenance to assure good system perfor-
mance, reliability and safety. Any modifications of spare parts or assemblies are only allowed with the
prior written permission of the manufacturer.
Modifications
Modifications to the device are only permitted after prior consultation and with the written approval
of the manufacturer. Modifications and upgrades shall only be carried out by an authorized BUCHI
technical engineer. The manufacturer will decline any claim resulting from unauthorized modifications.
3 Technical data
K-375 / K-376 / K-377 Operation Manual, Version F
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3 Technical data
This chapter introduces the reader to the device specifications. It contains the scope of delivery, tech-
nical data, requirements and performance data.
3.1 Scope of delivery
3.1.1 Basic devices
KjelMaster K-375 Order number
KjelMaster K-375
with glass splash protector and
potentiometric sensor
(220 – 240 V, 50/60 Hz)
113751700
KjelMaster K-375
with glass splash protector and
colorimetric sensor
(220 – 240 V, 50/60 Hz)
113752700
KjelMaster K-375
with plastic splash protector and
potentiometric sensor
(220 – 240 V, 50/60 Hz)
113753700
KjelMaster K-375
with plastic splash protector and
colorimetric sensor
(220 – 240 V, 50/60 Hz)
113754700
KjelSampler K-376 Order number
KjelSampler K-376
with one tray
(100 – 240 V, 50/60 Hz)
113750710
KjelSampler K-377 Order number
KjelSampler K-377
with two trays
(100 – 240 V, 50/60 Hz)
113750720
3 Technical data
K-375 / K-376 / K-377 Operation Manual, Version F
18
KjelMaster System K-375 / K-376 Order number
KjelMaster System K-375 / K-376
K-375 with glass splash protector and
potentiometric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376 / K-377: 100 – 240 V, 50/60 Hz
113751710
KjelMaster System K-375 / K-376
K-375 with glass splash protector and
colorimetric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376 / K-377: 100 – 240 V, 50/60 Hz
113752710
KjelMaster System K-375 / K-376
K-375 with plastic splash protector and
potentiometric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376 / K-377: 100 – 240 V, 50/60 Hz
113753710
KjelMaster System K-375 / K-376
K-375 with plastic splash protector and
colorimetric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376 / K-377: 100 – 240 V, 50/60 Hz
113754710
KjelMaster System K-375 / K-377 Order number
KjelMaster System K-375 / K-377
K-375 with glass splash protector and
potentiometric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376 / K-377: 100 – 240 V, 50/60 Hz
113751720
KjelMaster System K-375 / K-377
K-375 with glass splash protector and
colorimetric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376 / K-377: 100 – 240 V, 50/60 Hz
113752720
KjelMaster System K-375 / K-377
K-375 with plastic splash protector and
potentiometric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376 / K-377: 100 – 240 V, 50/60 Hz
113753720
KjelMaster System K-375 / K-377
K-375 with plastic splash protector and
colorimetric sensor
K-375: 220 – 240 V, 50/60 Hz
K-376 / K-377: 100 – 240 V, 50/60 Hz
113754720
3 Technical data
K-375 / K-376 / K-377 Operation Manual, Version F
19
3.1.2 Standard accessories for K-375
Description Order number Picture
Sample tube (300 mL) 1
Pair of glass tongs 002004 2
Connection cable RJ45 length 2 m 044989
Mains cable of the following types
Type CH
Type Schuko/Japan
Type GB
Type AUS
Type USA
010010
010016
017835
017836
033763
pH electrode
or (according to purchase order)
colorimetric sensor
Accessory kit for colorimetric sensor (if device version with colori-
metric sensor is shipped)
11056842
11066601
11068260
3
4
Indicator according to Sher, 100 mL (if device version with colori-
metric sensor is shipped)
003512 5
Buffer set pH 4 and pH 7, 3 x 20 mL each (if device version with
potentiometric sensor is shipped)
043188
KCI electrolyte, sat. , 250 mL (if device version with potentiometric
sensor is shipped)
11059759 6
Connection grommet for Chiller 049151 7
Hose connector in line 11–13 for waste tank 043178
Hose chemical supply, Nylflex, length 6 m, Ø 5/10 mm 043185
Suction tube to tanks, FEP, length 580 mm 043407
Hose waste drain, EPDM, L = 1.8 m, ø 11/18 mm 043457
Clamp D15.6 049167
Clamp D12.8 043297
Clamp D11.9 043841
Silicone hose ø 8 mm/12x1.8m 11058157
Y-piece ø12 mm 11058358
Cooling water hose complete: G 3/4”, G 1/2”, L = 1.5 m 037780
O-ring 190.1 x 3.53 EPDM 75 049676 8
O-ring 247.2 x 3.53 EPDM 11058241
3 Technical data
K-375 / K-376 / K-377 Operation Manual, Version F
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Description Order number Picture
FEP tube, 1.2 m, to driving motor 11056837
Capacitive level sensor for chemical or waste tank 11055914 9
Laboratory vessel 053203
Driving motor for dosing unit 11056835 10
Dosing unit (20 mL) 11056836 11
Test gauge sample tube holder 11059802 12
Tank 10 L 043410 13
Cap for 10 L tank, large 025869 14
Cap for 10 L and 20 L tank, small 043477 15
Tank labels 043434
Tank 20 L 043408 16
Cap for 20 L tank, large 043478 17
Distance holder for dosing tip 043203 18
Mini gender changer 043108
Weighing boats (20 pcs) 11060522
EPDM sealing for tanks 043048
Open end spanner 11058252 19
Tool SVL 22 11057779 20
CD KjelLink PC software (with 60 days test license) 11058664
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Buchi KjelMaster K-375 User manual

Type
User manual

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